Catalysts and methods for alcohol dehydration
a technology of aromatic alcohol and catalysts, which is applied in the direction of physical/chemical process catalysts, ether preparation by compound dehydration, ether preparation, etc., can solve the problems of less pure product, difficult handling, and potential cost, and achieve the effect of remarkable selectivity
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example 1
[0036]The synthesis of lanthanum oxychloride is carried out by thermal decomposition of LaCl3·7H2O. A sample of the powdered precursor (approximately 10 g) is calcined in air in a static calcination oven under the following temperature protocol: ramp 1.41° C. / min to 550° C., dwell 3 hrs at 550° C., cool down to room temperature. The elemental composition of the catalyst is assayed by X-ray fluorescence spectroscopy (XRF) to 17.23 wt. % chlorine, 69.63 wt. % lanthanum and 13.14 wt. % oxygen (balance). Thus, the elemental composition of the catalyst is La1.00O1.64Cl0.97. The specific surface area (BET) of the catalyst sample is measured to 6.2 m2 / g and its pore volume to 0.013 cm3 / g. The XRD data shows the presence of lanthanum oxychloride phases.
example 2
[0037]The lanthanum oxychloride catalyst from Example 1 is used for the dehydration of phenol. The powder is pressed and sieved to obtain particles that are between 0.60 mm and 0.85 mm in diameter. The particles are loaded into an electrically heated stainless steel reactor tube and heated to the reaction temperature with nitrogen flowing through the tube. After the reaction temperature is reached, vapor-phase phenol is passed through the reactor tube. The conversion of phenol is carried out at a weight hourly space velocity of 1 (WHSV=gram phenol / gram catalyst-hour) and at 500° C. Test conditions and results are shown in Table 1.
[0038]
TABLE 1ConversionSelectivity [mol. %]Test[mol. %]DiphenylConditionsPhenolOxideOPPDBFO-BIPPEM-BIPPEP-BIPPET = 500° C.0.70%95.86%0.02%4.12%0.00%0.00%0.00%Feed: PhOHToS = 1.5 hrsWHSV 1 hr−1T = 500° C.0.82%95.83%0.07%4.09%0.00%0.00%0.00%Feed: PhOHToS = 2.75 hrsWHSV 1 hr−1T = 500° C.0.82%95.90%0.18%3.93%0.00%0.00%0.00%Feed: PhOHToS = 3.75 hrsWHSV 1 hr−1T =...
example 3
[0039]A 1M LaCl3 solution, prepared by dissolving 50.00 g LaCl3 in 135 mL DI H2O, is added dropwise over 15 min into a 2L flask equipped with an overhead stirrer and an initial 500 mL DI H2O. The solution is stirred at 400 rpm with a 6 mm PTFE screw propeller blade. Approximately 182 mL of tetrapropylammonium hydroxide is added during the precipitation to keep the pH at a constant value of 9. The resulting white precipitate is allowed to age in solution for 1 h without stirring, after which time it is centrifuged at 7000 rpm for 5 min. The decanted precipitate is placed into an oven, dried at 120° C. for 4 h and calcined at 500° C. for 4 h with a ramp rate of 5° C. / min to give 23 g of product. Neutron activation analysis (NAA) reveals a total chlorine concentration of 5.8 wt %.
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